CN114437490B - Preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation - Google Patents
Preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation Download PDFInfo
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F259/00—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00
- C08F259/02—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing chlorine
- C08F259/04—Macromolecular compounds obtained by polymerising monomers on to polymers of halogen containing monomers as defined in group C08F14/00 on to polymers containing chlorine on to polymers of vinyl chloride
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- C08K3/38—Boron-containing compounds
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/38—Boron-containing compounds
- C08K2003/382—Boron-containing compounds and nitrogen
- C08K2003/385—Binary compounds of nitrogen with boron
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Abstract
The invention discloses a preparation method of modified polyvinyl chloride by gamma ray radiation, which comprises 3 steps of preparing a polyacrylamide grafted polyvinyl chloride material, preparing hydroxylated boron nitride and preparing the modified polyvinyl chloride material, wherein under the action of gamma rays, polyvinyl chloride and acrylamide monomers can generate a large amount of free radicals to generate polymerization reaction and crosslinking reaction, so as to obtain the polyacrylamide grafted polyvinyl chloride material, the polyacrylamide has the characteristic of high strength, and can be grafted on polyvinyl chloride to improve the mechanical property of the polyvinyl chloride, and meanwhile, the boron nitride has a soft lamellar structure.
Description
Technical Field
The invention relates to the technical field of preparation of polyvinyl chloride materials, in particular to a preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation.
Background
Polyvinyl chloride has the advantages of excellent chemical resistance, mechanical strength, electrical insulation, small flow resistance and the like. Polyvinyl chloride can be formed by extrusion, injection, molding, blow molding and the like, and is widely applied to manufacturing artificial leather, cables, plastic bags, films, daily necessities, various pipes and the like.
At present, the self-cleaning property, the mechanical property, the flame retardance, the low water vapor permeability, the anti-mildew property, the compatibility, the aging resistance, the oxidation resistance, the hydrophilicity and other properties of polyvinyl chloride materials need to be further improved, for example, patent document CN104231151B discloses a large-particle-size acrylate impact modifier for polyvinyl chloride and a preparation method thereof, wherein a seed emulsion polymerization process is adopted, polyvinyl alcohol is used as a protective colloid, a nucleation layer is a seed emulsion composed of butyl acrylate, isobornyl methacrylate, methyl methacrylate and a cross-linking agent, and a shell layer is formed by coating butyl acrylate, styrene, isobornyl methacrylate, methyl methacrylate and the cross-linking agent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation, which solves the technical problem that the mechanical property of the existing polyvinyl chloride material is poor.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation comprises the following specific steps:
(1) uniformly dispersing polyvinyl chloride powder in deionized water, adding an acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, then sending the solution into a cobalt 60 irradiation chamber for radiation, and after the radiation is finished, filtering, washing and drying a reaction product to obtain a polyacrylamide grafted polyvinyl chloride material;
(2) adding hexagonal boron nitride into a strong base solution, stirring in an oil bath, carrying out hydroxylation reaction, after the reaction is finished, washing and drying a reaction product to obtain hydroxylated boron nitride;
(3) and (3) uniformly mixing the polyacrylamide grafted polyvinyl chloride material obtained in the step (1) and the hydroxylated boron nitride obtained in the step (2) in a high-speed stirrer, then transferring the mixture to an irradiation chamber for radiation reaction, washing and drying a reaction product after the reaction is finished, and then placing the reaction product in a double-roll open mill for continuous press molding to obtain the modified polyvinyl chloride material.
Preferably, in the step (1), the mass ratio of the polyvinyl chloride to the acrylamide monomer is 8-12: 4-8.
Preferably, in the step (1), the irradiation dose is 20-40kGy, and the irradiation dose rate is 0.5-2 kGy/h.
Preferably, in the step (2), the strong alkali solution is a sodium hydroxide solution or a potassium hydroxide solution, and the concentration of the strong alkali solution is 4-8 mol/L.
Preferably, in the step (2), the dosage ratio of the hexagonal boron nitride to the strong base solution is 10-15g:200-300 mL.
Preferably, in the step (2), the oil bath temperature is 130-160 ℃, and the oil bath reaction time is 6-9 h.
Preferably, in the step (3), the mass ratio of the polyacrylamide grafted polyvinyl chloride to the hydroxylated boron nitride is 20-40: 5-8.
Preferably, in the step (3), the irradiation source is cobalt 60, the irradiation dose is 10-30kGy, and the irradiation dose rate is 0.2-1.5 kGy/h.
Preferably, in the step (3), the working temperature of the two-roll open mill is 160-180 ℃, and the mixing time is 5-10 min.
The invention also provides the modified polyvinyl chloride material prepared by the preparation method.
Compared with the prior art, the invention has the following beneficial effects:
(1) under the action of gamma rays, polyvinyl chloride and acrylamide monomers can generate a large amount of free radicals to generate polymerization reaction and crosslinking reaction, so that a polyacrylamide grafted polyvinyl chloride material is obtained, wherein polyacrylamide has the characteristic of high strength, and can be grafted on polyvinyl chloride to improve the mechanical property of the polyvinyl chloride;
(2) the boron nitride has a soft lamellar structure, is subjected to hydroxylation modification at first and then is grafted on the polyvinyl chloride, so that the problem of poor toughness of the polyvinyl chloride can be effectively solved, and the elongation at break and the impact strength of the polyvinyl chloride material are improved;
(3) according to the invention, the polyacrylamide grafted polyvinyl chloride material and the hydroxylated boron nitride are mixed and then subjected to radiation reaction, no catalyst or initiator is required to be added, the purity of the material is improved, and the elongation at break and the impact strength of the polyvinyl chloride material are further improved through the radiation reaction.
Detailed Description
The present invention will be described in more detail with reference to specific preferred embodiments, but the present invention is not limited to the following embodiments.
It should be noted that, unless otherwise specified, the chemical reagents involved in the present invention are commercially available.
The polyvinyl chloride powder adopted in the embodiment is purchased from Suhao speciality chemical company, Hebei, and the brand number is SG-5; hexagonal boron nitride was purchased from Shanghai Xiao Huan nanotechnology Co., Ltd, and had an average particle size of 80nm and a purity of > 99.9%.
Example 1
A preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation comprises the following preparation steps:
(1) uniformly dispersing 8g of polyvinyl chloride powder in 100mL of deionized water, adding 4g of acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, and then sending the solution into a cobalt 60 irradiation chamber for irradiation, wherein the irradiation dose is 20kGy, the irradiation dose rate is 0.5kGy/h, and after the irradiation is finished, filtering, washing and drying a reaction product to obtain the polyacrylamide grafted polyvinyl chloride material;
(2) adding 10g of hexagonal boron nitride into 200mL of 6mol/L sodium hydroxide solution, stirring in an oil bath at 130 ℃ for 6h, carrying out hydroxylation reaction, after the reaction is finished, washing and drying a reaction product to obtain hydroxylated boron nitride;
(3) uniformly mixing 20g of polyacrylamide grafted polyvinyl chloride material and 5g of hydroxylated boron nitride in a high-speed stirrer, then transferring the mixture to a cobalt 60 irradiation chamber for radiation reaction, wherein the irradiation dose is 10kGy, the irradiation dose rate is 0.2kGy/h, after the reaction is finished, washing and drying a reaction product, then placing the reaction product in a double-roll open mill, mixing for 6min at 160 ℃, and carrying out rolling forming to obtain the modified polyvinyl chloride material.
Example 2
A preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation comprises the following preparation steps:
(1) uniformly dispersing 10g of polyvinyl chloride powder in 100mL of deionized water, adding 5g of acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, and then sending the solution into a cobalt 60 irradiation chamber for irradiation, wherein the irradiation dose is 30kGy, the irradiation dose rate is 0.6kGy/h, and after the irradiation is finished, filtering, washing and drying a reaction product to obtain the polyacrylamide grafted polyvinyl chloride material;
(2) adding 15g of hexagonal boron nitride into 250mL of 6mol/L sodium hydroxide solution, stirring in an oil bath for 6 hours at 150 ℃, carrying out hydroxylation reaction, washing and drying a reaction product after the reaction is finished, thereby obtaining hydroxylated boron nitride;
(3) uniformly mixing 30g of polyacrylamide grafted polyvinyl chloride material and 5g of hydroxylated boron nitride in a high-speed stirrer, then transferring the mixture to a cobalt 60 irradiation chamber for radiation reaction, wherein the irradiation dose is 20kGy, the irradiation dose rate is 0.5kGy/h, after the reaction is finished, washing and drying a reaction product, then placing the reaction product in a double-roll open mill, mixing for 6min at 160 ℃, and carrying out rolling forming to obtain the modified polyvinyl chloride material.
Example 3
A preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation comprises the following preparation steps:
(1) uniformly dispersing 12g of polyvinyl chloride powder in 100mL of deionized water, adding 6g of acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, and then sending the solution into a cobalt 60 irradiation chamber for irradiation, wherein the irradiation dose is 25kGy, the irradiation dose rate is 1kGy/h, and after the irradiation is finished, filtering, washing and drying a reaction product to obtain the polyacrylamide grafted polyvinyl chloride material;
(2) adding 12g of hexagonal boron nitride into 250mL of 5mol/L sodium hydroxide solution, stirring in an oil bath at 160 ℃ for 6h, carrying out hydroxylation reaction, after the reaction is finished, washing and drying a reaction product to obtain hydroxylated boron nitride;
(3) uniformly mixing 35g of polyacrylamide grafted polyvinyl chloride material and 8g of hydroxylated boron nitride in a high-speed stirrer, then transferring the mixture to a cobalt 60 irradiation chamber for radiation reaction, wherein the irradiation dose is 25kGy, the irradiation dose rate is 1kGy/h, after the reaction is finished, washing and drying a reaction product, then placing the reaction product in a double-roll open mill, mixing for 8min at 160 ℃, and carrying out rolling forming to obtain the modified polyvinyl chloride material.
Example 4
A preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation comprises the following preparation steps:
(1) uniformly dispersing 10g of polyvinyl chloride powder in 100mL of deionized water, adding 8g of acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, and then sending the solution into a cobalt 60 irradiation chamber for irradiation, wherein the irradiation dose is 40kGy, the irradiation dose rate is 2kGy/h, and after the irradiation is finished, filtering, washing and drying a reaction product to obtain the polyacrylamide grafted polyvinyl chloride material;
(2) adding 15g of hexagonal boron nitride into 250mL of 8mol/L sodium hydroxide solution, stirring in an oil bath for 8 hours at 150 ℃, carrying out hydroxylation reaction, washing and drying a reaction product after the reaction is finished, thereby obtaining hydroxylated boron nitride;
(3) uniformly mixing 40g of polyacrylamide grafted polyvinyl chloride material and 6g of hydroxylated boron nitride in a high-speed stirrer, then transferring the mixture to a cobalt 60 irradiation chamber for radiation reaction, wherein the irradiation dose is 30kGy, the irradiation dose rate is 1.5kGy/h, after the reaction is finished, washing and drying a reaction product, then placing the reaction product in a double-roll open mill, mixing for 6min at 180 ℃, and carrying out rolling forming to obtain the modified polyvinyl chloride material.
Comparative example 1
A preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation comprises the following preparation steps:
(1) adding 12g of hexagonal boron nitride into 250mL of 5mol/L sodium hydroxide solution, stirring in an oil bath for 6 hours at 160 ℃, carrying out hydroxylation reaction, washing and drying a reaction product after the reaction is finished, thereby obtaining hydroxylated boron nitride;
(2) uniformly mixing 35g of polyvinyl chloride powder and 8g of hydroxylated boron nitride in a high-speed stirrer, transferring the mixture to a cobalt 60 irradiation chamber for radiation reaction, wherein the irradiation dose is 25kGy, the irradiation dose rate is 1kGy/h, after the reaction is finished, washing and drying a reaction product, then placing the reaction product in a double-roll open mill, mixing for 8min at 160 ℃, and carrying out rolling forming to obtain the modified polyvinyl chloride material.
Comparative example 2
A preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation comprises the following preparation steps:
(1) uniformly dispersing 12g of polyvinyl chloride powder in 100mL of deionized water, adding 6g of acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, and then sending the solution into a cobalt 60 irradiation chamber for irradiation, wherein the irradiation dose is 25kGy, the irradiation dose rate is 1kGy/h, and after the irradiation is finished, filtering, washing and drying a reaction product to obtain the polyacrylamide grafted polyvinyl chloride material;
(2) uniformly mixing 35g of polyacrylamide grafted polyvinyl chloride material and 8g of boron nitride in a high-speed stirrer, then transferring the mixture to a cobalt 60 irradiation chamber for radiation reaction, wherein the irradiation dose is 25kGy, and the irradiation dose rate is 1kGy/h, after the reaction is finished, washing and drying a reaction product, then placing the reaction product in a double-roll open mill, mixing for 8min at 160 ℃, and carrying out rolling forming to obtain the modified polyvinyl chloride material.
Comparative example 3
A preparation method of modified polyvinyl chloride comprises the following preparation steps:
(1) uniformly dispersing 12g of polyvinyl chloride powder in 100mL of deionized water, adding 6g of acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, and then sending the solution into a cobalt 60 irradiation chamber for irradiation, wherein the irradiation dose is 25kGy, the irradiation dose rate is 1kGy/h, and after the irradiation is finished, filtering, washing and drying a reaction product to obtain the polyacrylamide grafted polyvinyl chloride material;
(2) adding 12g of hexagonal boron nitride into 250mL of 5mol/L sodium hydroxide solution, stirring in an oil bath at 160 ℃ for 6h, carrying out hydroxylation reaction, after the reaction is finished, washing and drying a reaction product to obtain hydroxylated boron nitride;
(3) uniformly mixing 35g of polyacrylamide grafted polyvinyl chloride material and 8g of hydroxylated boron nitride in a high-speed stirrer, then placing the mixture in a double-roll open mill, mixing for 8min at 160 ℃, and carrying out rolling forming to obtain the modified polyvinyl chloride material.
Placing the modified polyvinyl chloride materials prepared in the examples 1-4 and the comparative examples 1-3 in a tablet press, setting the temperature of the tablet press to 180 ℃, pressing for 10min to obtain a sheet with the thickness of 4mm, cooling to room temperature to obtain a test sample, and then testing the test sample, wherein the specific steps are as follows:
the notch impact strength is tested according to the national standard GB/T1043.1-2008, the temperature is 25 ℃, the V-shaped notch is formed, the size of a sample is 80mm multiplied by 10mm multiplied by 4mm, the notch depth is 2mm, and the test instrument is as follows: an XJJ-50 type simply supported beam impact tester;
the elongation at break is tested according to GB/T1040.1-2018, the clamping distance of the dumbbell-shaped test sample is 25.0 +/-1.0 mm, the material stretching speed is 50mm/min, and the test instrument: MTS universal tester;
flexural strength was tested according to GB/T9341-: the sample size is 80mm × 10mm × 4mm, the bending speed is 2mm/min, the test apparatus: ST-S501 bending performance testing machine;
the tensile strength is tested according to GB/T1040.1-2018, the tensile speed is 10mm/min, and the tensile strength is measured by a test instrument: MTS universal tester; the test results are shown in the following table:
finally, it is to be noted that: the above examples do not limit the invention in any way. It will be apparent to those skilled in the art that various modifications and improvements can be made to the present invention. Accordingly, any modification or improvement made without departing from the spirit of the present invention is within the scope of the claimed invention.
Claims (10)
1. A preparation method for modifying polyvinyl chloride by utilizing gamma ray radiation is characterized by comprising the following specific steps:
(1) uniformly dispersing polyvinyl chloride powder in deionized water, adding an acrylamide monomer, performing ultrasonic dispersion uniformly, introducing nitrogen into the solution to remove oxygen in the mixed solution, sealing, then sending the solution into a cobalt 60 irradiation chamber for radiation, and after the radiation is finished, filtering, washing and drying a reaction product to obtain a polyacrylamide grafted polyvinyl chloride material;
(2) adding hexagonal boron nitride into a strong base solution, stirring in an oil bath, carrying out hydroxylation reaction, after the reaction is finished, washing and drying a reaction product to obtain hydroxylated boron nitride;
(3) and (3) uniformly mixing the polyacrylamide grafted polyvinyl chloride material obtained in the step (1) and the hydroxylated boron nitride obtained in the step (2) in a high-speed stirrer, then transferring the mixture to an irradiation chamber for radiation reaction, washing and drying a reaction product after the reaction is finished, and then placing the reaction product in a double-roll open mill for continuous press molding to obtain the modified polyvinyl chloride material.
2. The method for preparing polyvinyl chloride modified by gamma-ray irradiation according to claim 1, wherein the mass ratio of polyvinyl chloride to acrylamide monomer in step (1) is 8-12: 4-8.
3. The method for preparing polyvinyl chloride modified by gamma-ray irradiation according to claim 1, wherein in the step (1), the irradiation dose is 20-40kGy and the irradiation dose rate is 0.5-2 kGy/h.
4. The method for preparing polyvinyl chloride modified by gamma-ray irradiation according to claim 1, wherein in the step (2), the strong alkali solution is sodium hydroxide solution or potassium hydroxide solution, and the concentration of the strong alkali solution is 4-8 mol/L.
5. The method as claimed in claim 1, wherein the amount of the hexagonal boron nitride to the strong alkali solution in step (2) is 10-15g:200-300 mL.
6. The method for preparing polyvinyl chloride modified by gamma-ray irradiation as claimed in claim 1, wherein in step (2), the oil bath temperature is 130-160 ℃ and the oil bath reaction time is 6-9 h.
7. The method for preparing polyvinyl chloride modified by gamma-ray irradiation according to claim 1, wherein in the step (3), the mass ratio of the polyacrylamide grafted polyvinyl chloride to the hydroxylated boron nitride is 20-40: 5-8.
8. The method for preparing gamma-ray radiation modified polyvinyl chloride according to claim 1, wherein in the step (3), the radiation source is cobalt 60, the radiation dose is 10-30kGy, and the radiation dose rate is 0.2-1.5 kGy/h.
9. The method as claimed in claim 1, wherein the two-roll mill is operated at 160-180 deg.C for 5-10min in step (3).
10. A modified polyvinyl chloride material obtained by the production process as claimed in any one of claims 1 to 9.
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